Double salts of antimony



UNITED STATES PATENT OFFICE...

OSCAR O. FROELICH OF JERSEY CITY, NEW JERSEY.

DOUBLE SALTS OF ANTIMONY.

SPECIFICATION forming part of Letters PatentNo. 532,150, dated January8, 1895. Application filed March 6, 1894. Serial No. 502,564. (Nospecimens.)

To all whom it may concern.-

Be it known that I, OSCAR 0. B. FROELICH, a resident of Jersey City,Hudson county, and State of New Jersey, have discovered certain new anduseful Double Salts of Antimonynamely, the compounds of fluorid ofantimony (SbFl with the oxalates of antimony and alkali used asm'ordants for dyeing purposes-of which the following is a specificaion.

My invention consists broadly in a new compound consisting of a doublesalt of .fluorid and oxalate of antimony and alkali.

Up to the present time the only known compounds of fluorid of antimonyare either with the sulfates, or fluorids or chlorids of alkalies. Ihave succeeded in combining the fiuorid of antimony with other antimonysalts, the acid of which is oxalic acid, an organic acid, as such, andfor other reasons later mentioned, is much preferable to mineral acids.

These new compounds generally contain,

according to analyses, one molecule of fluorid of antimony to onemolecule of oxalic acid. Therefore the difierent known oxalates, theformulas of which have from one to live molecules of oxalic acid to onemolecule of antimony (SbO) are able to combine with fiuorid of antimonymolecule for molecule.

The chemical constitution of some of these new compounds is as follows:I

having a percentage of sixty-five to sixty-six per cent. antimony oxid.and lower, according to the percentage of antimony oxid of the oxalateapplied for combination. In these formulae M represents the alkalimetal, which of course includes ammonium.

These compounds are well formed crystals, readily and completely solublein Warm Water, and on account of their composition show, when applied asmordant, in a more pronounced manner all the good qualities of thedouble oxalate of antimony and potash (C O )''SbOK H +aq., which,according to authorities, gives results equal to those of tartar emetic,although containing only about half the percentage of antimony oxid.This arises from thefact thatoxalicacid separatesquicker and morecompletely from the latter.

These new compounds contain more than double the quantity of antimonyoxid than is contained in oxalate of antimony and more than in tartaremetic and many other antimony salts which are in use at present,develop less free hydrofluoric acid, are therefore not so injurious tothe fibers and transfer the oxid quicker and more completely to tannicacid on the fiber, being thus a pronounced improvement over othercompounds.

These compounds may be variously produced by various methods, some ofwhich are as follows, it being understood that I in no sense limitmyself to any specific method,

stating forth these merely as examples of some specific methods offorming my improved double'salts: I saturate a mixture of hydrofluoricacid and oxalic acid, in the proportion of three molecules ofhydrofluoric acid (I-IFl) to one molecule of oxalic acid (C O Hgradually adding alkalies to the boiling mixture, until neutralized,that is, until antimony oxid commences to precipitate. I then filter thesolution and cool down to crystallization. In practice. I take aboutsixty pounds of antimony oxid, thirty-six pounds of hydrofluoric acid offifty per cent. (HFl,) thirty-six pounds of oxalic acid crystals, andtwenty-eight pounds hydrate of potash, which yield about one hundred andtwenty pounds fine soluble crystals containing about fifty per cent.antimony oxid. These specific proportions, as well as the proportionslater specified, may, however, be varied without departing from thespirit of my invention.

Although my improved compound may be made as above, I prefer to makesolutions in water of fiuorid of antimony (SbFl and of oxalate ofantimony and alkali, all prepared separately after known methods, and tocombine these afterward always, by preference, in the proportion of onemolecule of oxalic acid to three molecules of hydrofluoric acidl Asurplus of fluorid, however, does no harm, as it is only essential forgetting completely soluble crystals to have the solutions as neutral aspossible without precipitating antimony oxid. The mixed solutions oncooling down and further evaporation, yield almost IOOtheoretioalquantities of small but well-formed glittering crystals infine needles or columns. For instance, ten pounds hydrofluoric acidfifty per cent. saturated with (Sb O (equal to about fifteen poundsfluorid of antimony) mixed with a neutralized solution of ten poundsbinoxalate of potash saturated with (Sb O (equal to about one andone-third pounds oxalate of antimony), yield about 10 twenty-five poundsfine soluble crystals.

Having now described my invention, what I claim is r As a new antimonymordant, the soluble compound of fiuorid of antimony (SbFI with a doubleoxalate of antimony and alkali, sub- I 5 stantially as described.

. OSCAR O. B. FROELICH. Witnesses:

HARRY M. TURK, GEO. E. MORSE.

